CN106495227A - A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder - Google Patents
A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder Download PDFInfo
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Abstract
A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, it is related to a kind of nano-manganese dioxide raw powder's production technology.The invention aims to the manganese dioxide for solving existing method preparation is not oil-soluble, the manganese dioxide size of preparation is big, the problem that easily reunites.Method：First, liquor potassic permanganate is prepared；2nd, hydrogenperoxide steam generator is prepared；3rd, hydrogenperoxide steam generator is added dropwise in liquor potassic permanganate, sedimentation agent is added after stirring reaction, be stirred for reacting；Carry out again lowering the temperature, stand, clean, drying, grinding, obtain oil-soluble dispersed nano manganese dioxide powder.The present invention prepare oil-soluble dispersed nano manganese dioxide powder particle diameter be 1nm～80nm, the present invention can obtain the crystal formation and pattern that size is little, mono-dispersed nano manganese dioxide is stable.The present invention is suitable for preparing oil-soluble dispersed nano manganese dioxide powder.
Description
Technical field
The present invention relates to a kind of nano-manganese dioxide raw powder's production technology.
Background technology
Manganese dioxide is a kind of quite varied inorganic amphoteric oxide of purposes, due to the physicochemical characteristics for having uniqueness,
Preparation process is simple, cost is relatively low, abundant raw materials, the low reason of environmental pollution are widely used.Such as：Use in chemical reaction
Make catalyst, serve as polarization agent, biological molecular sieve, energy storage medium, lithium ion battery, ultracapacitor, glass in the battery
Good decolorising agent etc. in glass industry, can be also used for pyrotechnics, water purification except iron, medicine, fertilizer and fabric printing, paint and
The drier of ink.Therefore the preparation technology of research manganese dioxide has been applied to vital effect.And nanoscale dioxy
Change manganese because of the granular of its particle size, specific surface area increases severely and generates the effect of the surface not available for conventional manganese bioxide material
Should, size dimension effect, i.e. surface area increase, and activity centre increases, and reacting environment increases, and can increase electric discharge in electrode reaction
Capacity.It is likely to play more preferable catalytic action in chemical reaction.
Therefore, the scientists numerous studies preparation technology of manganese dioxide.But manganese dioxide prepared by existing method is not
It is oil-soluble, size is big, and manganese dioxide is easily reunited.
Content of the invention
The invention aims to the manganese dioxide for solving existing method preparation is not oil-soluble, the manganese dioxide of preparation
Size is big, the problem that easily reunites, and provides a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder.
A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, is completed according to the following steps：
First, potassium permanganate is dissolved in distilled water, obtains liquor potassic permanganate；
The mass fraction of the liquor potassic permanganate described in step one is 3%～10%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the mistake that mass fraction is 2%～5%
Hydrogen peroxide solution；
3rd, the liquor potassic permanganate obtained in step one is heated to 35 DEG C～50 DEG C, then is 35 DEG C～50 DEG C to temperature
Liquor potassic permanganate in the rate of addition of 5 drop/min～15 drop/min be added dropwise mass fraction that step 2 obtains as 2%～
5% hydrogenperoxide steam generator；Obtain reactant liquor；Reactant liquor is warming up to 75 DEG C～85 DEG C, then temperature be 75 DEG C～85 DEG C and
Mixing speed is stirring reaction 5min～15min under 300r/min～800r/min, then adds sedimentation agent in reactant liquor, then
It is stirring reaction 40min～60min under 300r/min～800r/min with mixing speed that temperature is 75 DEG C～85 DEG C；
In reactant liquor described in step 3, potassium permanganate is 1 with the mol ratio of hydrogen peroxide:(1.5～2.5)；
The quality of the sedimentation agent described in step 3 is (0.1g～1g) with the volume ratio of reactant liquor:100mL；
4th, low whipping speed is will to be reacted with the cooling rate of 2 DEG C/min～5 DEG C/min under 300r/min～800r/min
The temperature of liquid is down to 30 DEG C～35 DEG C from 75 DEG C～85 DEG C, then stops stirring, and stands 10min～20min；Upper strata after by standing
Clear liquid is poured out, and filters the MnO of lower floor2, solid matter after being filtered；Using the water that temperature is 85 DEG C～95 DEG C to filtration after
Solid matter clean 3 times～5 times, reuse methyl alcohol clean 2 times～4 times, the MnO after being cleaned2Powder；
5th, by cleaning after MnO2Powder is to dry 2h～5h at 25 DEG C～35 DEG C in temperature, then is ground, and obtains oil
Dissolubility dispersed nano manganese dioxide powder；
The particle diameter of the oil-soluble dispersed nano manganese dioxide powder described in step 5 is 1nm～80nm.
The principle and advantage of the present invention：
First, reaction equation of the invention is：
2MnO4 -+4H2O2→2MnO2+2H2O+5O2(g)+2OH-；
2nd, on the one hand the sedimentation agent that the present invention is added can make MnO2Little particle is easily separated from the aqueous solution, another
Aspect, prevents the reunion of nano particle, particle size distribution from can narrow, improves the stability of powder, expands which and applies neck
Domain；
3rd, the oil-soluble dispersed nano manganese dioxide powder and existing manganese dioxide powder body phase ratio that prepared by the present invention, system
Standby process is simple, low cost, particle size distribution are narrow, due to the stability of the powder that the cladding of oleic acid is improved so as to which application becomes
Obtain more extensive；
4th, the present invention prepare oil-soluble dispersed nano manganese dioxide powder particle diameter be 1nm～80nm, present invention side
Method can obtain the crystal formation and pattern that size is little, mono-dispersed nano manganese dioxide is stable；
5th, method of the present invention process is simple, so that the application of nano-manganese dioxide is wider so as to which performance is whole
Show.
The present invention is suitable for preparing oil-soluble dispersed nano manganese dioxide powder.
Description of the drawings
Fig. 1 is the SEM figures of the oil-soluble dispersed nano manganese dioxide powder prepared in one step 5 of embodiment.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder
Complete according to the following steps：
First, potassium permanganate is dissolved in distilled water, obtains liquor potassic permanganate；
The mass fraction of the liquor potassic permanganate described in step one is 3%～10%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the mistake that mass fraction is 2%～5%
Hydrogen peroxide solution；
3rd, the liquor potassic permanganate obtained in step one is heated to 35 DEG C～50 DEG C, then is 35 DEG C～50 DEG C to temperature
Liquor potassic permanganate in the rate of addition of 5 drop/min～15 drop/min be added dropwise mass fraction that step 2 obtains as 2%～
5% hydrogenperoxide steam generator；Obtain reactant liquor；Reactant liquor is warming up to 75 DEG C～85 DEG C, then temperature be 75 DEG C～85 DEG C and
Mixing speed is stirring reaction 5min～15min under 300r/min～800r/min, then adds sedimentation agent in reactant liquor, then
It is stirring reaction 40min～60min under 300r/min～800r/min with mixing speed that temperature is 75 DEG C～85 DEG C；
In reactant liquor described in step 3, potassium permanganate is 1 with the mol ratio of hydrogen peroxide:(1.5～2.5)；
The quality of the sedimentation agent described in step 3 is (0.1g～1g) with the volume ratio of reactant liquor:100mL；
4th, low whipping speed is will to be reacted with the cooling rate of 2 DEG C/min～5 DEG C/min under 300r/min～800r/min
The temperature of liquid is down to 30 DEG C～35 DEG C from 75 DEG C～85 DEG C, then stops stirring, and stands 10min～20min；Upper strata after by standing
Clear liquid is poured out, and filters the MnO of lower floor2, solid matter after being filtered；Using the water that temperature is 85 DEG C～95 DEG C to filtration after
Solid matter clean 3 times～5 times, reuse methyl alcohol clean 2 times～4 times, the MnO after being cleaned2Powder；
5th, by cleaning after MnO2Powder is to dry 2h～5h at 25 DEG C～35 DEG C in temperature, then is ground, and obtains oil
Dissolubility dispersed nano manganese dioxide powder；
The particle diameter of the oil-soluble dispersed nano manganese dioxide powder described in step 5 is 1nm～80nm.
The principle and advantage of present embodiment：
First, the reaction equation of present embodiment is：
2MnO4 -+4H2O2→2MnO2+2H2O+5O2(g)+2OH-；
2nd, on the one hand the sedimentation agent that present embodiment is added can make MnO2Little particle is easily separated from the aqueous solution,
On the other hand, prevent the reunion of nano particle, particle size distribution from can narrow, improve the stability of powder, expanding which should
Use field；
3rd, the oil-soluble dispersed nano manganese dioxide powder and existing manganese dioxide powder body phase that prepared by present embodiment
Than preparation process is simple, low cost, particle size distribution are narrow, due to the stability of the powder that the cladding of oleic acid is improved so as to should
With becoming more extensive；
4th, present embodiment prepare oil-soluble dispersed nano manganese dioxide powder particle diameter be 1nm～80nm, this reality
Apply methods and can obtain the crystal formation and pattern that size is little, mono-dispersed nano manganese dioxide is stable；
5th, the method process is simple of present embodiment, so that the application of nano-manganese dioxide is wider so as to performance
All show.
Present embodiment is suitable for preparing oil-soluble dispersed nano manganese dioxide powder.
Specific embodiment two：Present embodiment with one difference of specific embodiment is：Gao Meng described in step one
The mass fraction of sour potassium solution is 3%～5%.Other steps are identical with specific embodiment one.
Specific embodiment three：Present embodiment with one of specific embodiment one or two difference is：Institute in step one
The mass fraction of the liquor potassic permanganate that states is 5%～10%.Other steps are identical with specific embodiment one or two.
Specific embodiment four：Present embodiment with one of specific embodiment one to three difference is：Will in step 2
Mass fraction is that 30% hydrogenperoxide steam generator is diluted, and obtains the hydrogenperoxide steam generator that mass fraction is 2%～3%.Its
His step is identical with specific embodiment one to three.
Specific embodiment five：Present embodiment with one of specific embodiment one to four difference is：Will in step 2
Mass fraction is that 30% hydrogenperoxide steam generator is diluted, and obtains the hydrogenperoxide steam generator that mass fraction is 3%～5%.Its
His step is identical with specific embodiment one to four.
Specific embodiment six：Present embodiment with one of specific embodiment one to five difference is：Institute in step 3
In the reactant liquor that states, potassium permanganate is 1 with the mol ratio of hydrogen peroxide:2.Other steps are identical with specific embodiment one to five.
Specific embodiment seven：Present embodiment with one of specific embodiment one to six difference is：Institute in step 3
The sedimentation agent that states is oleic acid or oleyl amine.Other steps are identical with specific embodiment one to six.
Specific embodiment eight：Present embodiment with one of specific embodiment one to seven difference is：Will in step 3
The liquor potassic permanganate obtained in step one is heated to 40 DEG C, then in the liquor potassic permanganate that temperature is 40 DEG C with 10 drops/min
Rate of addition the hydrogenperoxide steam generator that the mass fraction that obtains of step 2 is 3% is added dropwise；Obtain reactant liquor；Reactant liquor is heated up
To 80 DEG C, then temperature be 80 DEG C and mixing speed be stirring reaction 10min under 500r/min, then add sedimentation in reactant liquor
Agent, then temperature be 80 DEG C and mixing speed be stirring reaction 60min under 500r/min.Other steps and specific embodiment one
Identical to seven.
Specific embodiment nine：Present embodiment with one of specific embodiment one to eight difference is：In step 4
Mixing speed is that the temperature of reactant liquor is down to 30 DEG C from 80 DEG C with the cooling rate of 3 DEG C/min under 500r/min, then stops stirring
Mix, stand 10min；Supernatant liquor after by standing is poured out, and filters the MnO of lower floor2, solid matter after being filtered；Use
Temperature be 90 DEG C of water to filtration after solid matter clean 3 times, reuse methyl alcohol and clean 2 times, the MnO after being cleaned2Powder
End.Other steps are identical with specific embodiment one to eight.
Specific embodiment ten：Present embodiment with one of specific embodiment one to nine difference is：Institute in step 5
The particle diameter of the oil-soluble dispersed nano manganese dioxide powder that states is 20nm.Other steps and one to nine phase of specific embodiment
With.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, is to complete according to the following steps
's：
First, potassium permanganate is dissolved in distilled water, obtains liquor potassic permanganate；
The mass fraction of the liquor potassic permanganate described in step one is 5%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the hydrogen peroxide that mass fraction is 3%
Solution；
3rd, the liquor potassic permanganate obtained in step one is heated to 40 DEG C, then molten to the potassium permanganate that temperature is 40 DEG C
The mass fraction obtained with the rate of addition dropwise addition step 2 of 10 drop/min in liquid is 3% hydrogenperoxide steam generator；Reacted
Liquid；Reactant liquor is warming up to 80 DEG C, then temperature be 80 DEG C and mixing speed be stirring reaction 10min under 500r/min, then to
Add sedimentation agent in reactant liquor, then temperature be 80 DEG C and mixing speed be stirring reaction 60min under 500r/min；
In reactant liquor described in step 3, potassium permanganate is 1 with the mol ratio of hydrogen peroxide:2.5；
The quality of the sedimentation agent described in step 3 is 1g with the volume ratio of reactant liquor:100mL；
4th, low whipping speed is to be down to the temperature of reactant liquor from 80 DEG C with the cooling rate of 3 DEG C/min under 500r/min
30 DEG C, then stop stirring, stand 10min；Supernatant liquor after by standing is poured out, and filters the MnO of lower floor2, after being filtered
Solid matter；Using the water that temperature is 90 DEG C to filtration after solid matter clean 3 times, reuse methyl alcohol and clean 2 times, obtain clear
MnO after washing2Powder；
5th, by cleaning after MnO2Powder is to dry 4h at 30 DEG C in temperature, then is ground, and obtains oil-soluble single dispersing
Nano-manganese dioxide powder；
The particle diameter of the oil-soluble dispersed nano manganese dioxide powder described in step 5 is 20nm.
Fig. 1 is the SEM figures of the oil-soluble dispersed nano manganese dioxide powder prepared in one step 5 of embodiment, from Fig. 1
Understand, the particle diameter of oil-soluble dispersed nano manganese dioxide powder prepared by embodiment one is about 20nm, size is little, and pattern is equal
One.
Oil-soluble dispersed nano manganese dioxide powder prepared by embodiment one can be applied and make depolarizing agent in the battery,
The aspects such as the decolorising agent in glass industry, the drier of the catalyst of organic synthesis, paint and ink, fabric printing agent；Due to
Size is little, and shape is homogeneous, can reach the effect of repid discharge when applied after surface treatment in the battery；Catalysis in organic synthesis
Efficiency also has very high lifting；Application in coating and printing and dyeing is that have organic dispersiveness well.
Claims (10)
1. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, it is characterised in that a kind of oil-soluble single dispersing is received
The preparation method of rice manganese dioxide powder is completed according to the following steps：
First, potassium permanganate is dissolved in distilled water, obtains liquor potassic permanganate；
The mass fraction of the liquor potassic permanganate described in step one is 3%～10%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the peroxidating that mass fraction is 2%～5%
Hydrogen solution；
3rd, the liquor potassic permanganate obtained in step one is heated to 35 DEG C～50 DEG C, then to the height that temperature is 35 DEG C～50 DEG C
The mass fraction obtained with the rate of addition dropwise addition step 2 of 5 drop/min～15 drop/min in potassium manganate solution is 2%～5%
Hydrogenperoxide steam generator；Obtain reactant liquor；Reactant liquor is warming up to 75 DEG C～85 DEG C, then is 75 DEG C～85 DEG C and stirring speed in temperature
Spend for stirring reaction 5min under 300r/min～800r/min～15min, then sedimentation agent is added in reactant liquor, then in temperature be
75 DEG C～85 DEG C is stirring reaction 40min～60min under 300r/min～800r/min with mixing speed；
In reactant liquor described in step 3, potassium permanganate is 1 with the mol ratio of hydrogen peroxide:(1.5～2.5)；
The quality of the sedimentation agent described in step 3 is (0.1g～1g) with the volume ratio of reactant liquor:100mL；
4th, low whipping speed is by reactant liquor under 300r/min～800r/min with the cooling rate of 2 DEG C/min～5 DEG C/min
Temperature is down to 30 DEG C～35 DEG C from 75 DEG C～85 DEG C, then stops stirring, and stands 10min～20min；Supernatant liquor after by standing
Pour out, filter the MnO of lower floor2, solid matter after being filtered；Using the water that temperature is 85 DEG C～95 DEG C to filtration after consolidate
Body material is cleaned 3 times～5 times, is reused methyl alcohol and is cleaned 2 times～4 times, the MnO after being cleaned2Powder；
5th, by cleaning after MnO2Powder is to dry 2h～5h at 25 DEG C～35 DEG C in temperature, then is ground, and obtains oil-soluble
Dispersed nano manganese dioxide powder；
The particle diameter of the oil-soluble dispersed nano manganese dioxide powder described in step 5 is 1nm～80nm.
2. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The mass fraction of the liquor potassic permanganate described in step one is 3%～5%.
3. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The mass fraction of the liquor potassic permanganate described in step one is 5%～10%.
4. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The hydrogenperoxide steam generator that mass fraction is 30% is diluted in step 2, obtains the peroxide that mass fraction is 2%～3%
Change hydrogen solution.
5. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The hydrogenperoxide steam generator that mass fraction is 30% is diluted in step 2, obtains the peroxide that mass fraction is 3%～5%
Change hydrogen solution.
6. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
In reactant liquor described in step 3, potassium permanganate is 1 with the mol ratio of hydrogen peroxide:2.
7. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
Sedimentation agent described in step 3 is oleic acid or oleyl amine.
8. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The liquor potassic permanganate obtained in step one is heated to 40 DEG C in step 3, then to the liquor potassic permanganate that temperature is 40 DEG C
In the hydrogenperoxide steam generator that the mass fraction that step 2 obtains is 3% is added dropwise with the rate of addition of 10 drop/min；Obtain reactant liquor；
Reactant liquor is warming up to 80 DEG C, then temperature be 80 DEG C and mixing speed be stirring reaction 10min under 500r/min, then to reaction
Add sedimentation agent in liquid, then temperature be 80 DEG C and mixing speed be stirring reaction 60min under 500r/min.
9. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
In step 4, low whipping speed is that the temperature of reactant liquor is down to 30 from 80 DEG C with the cooling rate of 3 DEG C/min under 500r/min
DEG C, then stop stirring, stand 10min；Supernatant liquor after by standing is poured out, and filters the MnO of lower floor2, consolidating after being filtered
Body material；Using the water that temperature is 90 DEG C to filtration after solid matter clean 3 times, reuse methyl alcohol clean 2 times, cleaned
MnO afterwards2Powder.
10. the preparation method of a kind of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The particle diameter of the oil-soluble dispersed nano manganese dioxide powder described in step 5 is 20nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109796048A (en) * | 2019-03-27 | 2019-05-24 | 中国人民解放军陆军工程大学 | Controlled synthesis method of manganese dioxide with different crystal forms |
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| CN1515632A (en) * | 2003-08-26 | 2004-07-28 | 武汉理工大学 | Preparation method of inorganic-organic composite particle and its special-purpose equipment |
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| CN1515632A (en) * | 2003-08-26 | 2004-07-28 | 武汉理工大学 | Preparation method of inorganic-organic composite particle and its special-purpose equipment |
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| CN109796048A (en) * | 2019-03-27 | 2019-05-24 | 中国人民解放军陆军工程大学 | Controlled synthesis method of manganese dioxide with different crystal forms |
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